A polyhedral oligomeric silsesquioxane containing hydroxyl metal tin and its preparation and application
A polysilsesquioxane, polyhedral technology, applied in the field of polyhedral oligomeric silsesquioxane, can solve the problem of no research on polymerization catalysts and the like
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[0039] Another aspect of the present invention provides a method for preparing polyhedral oligosilsesquioxane containing hydroxyl metal tin, preferably the method for preparing the polyhedral oligomeric silsesquioxane containing hydroxyl metal tin described in the first aspect of the present invention , the method includes the following steps:
[0040] Step 1, mixing hydroxyl-containing polyhedral oligomeric silsesquioxane, an organotin compound and a solvent;
[0041] According to the present invention, in step 1, the hydroxyl-containing polyhedral oligomeric silsesquioxane is preferably the hydroxyl-containing polyhedral oligomeric silsesquioxane described in the first aspect of the present invention.
[0042] According to the present invention, in step 1, the organotin compound is preferably the organotin compound described in the first aspect of the present invention.
[0043] In the present invention, the reaction system needs to be carried out in an anhydrous environmen...
Embodiment approach
[0070] According to a preferred embodiment of the present invention, the polyhedral oligomeric silsesquioxane containing hydroxyl metal tin can be prepared by any of the following processes:
[0071]
[0072] In formula (9), R is selected from alkyl, phenyl or substituted phenyl, wherein, alkyl is selected from C 1 -C 16 Alkyl group, preferably C 1 -C 8 The alkyl group, more preferably one or more of methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl and tert-butyl, for example, R is selected from methyl, n-butyl or phenyl.
[0073]
[0074] In formula (10), R is selected from alkyl, phenyl or substituted phenyl, wherein, alkyl is selected from C 1 -C 16 Alkyl group, preferably C 1 -C 8 The alkyl group, more preferably one or more of methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl and tert-butyl, for example, R is selected from methyl, n-butyl or phenyl.
[0075]
[0076] In formula (11), R is selected from alkyl, phenyl or substituted phenyl, wherei...
Embodiment 1
[0106] 2.00g (1.87mmol) Tetrasilanolpheny POSS is joined in the 50ml reaction flask, then the reaction flask is continuously pumped and vacuumed three times, feeds nitrogen, makes the whole reaction system under the nitrogen environment, dissolves 1.22g (3.74mmol) of toluene solvent ) Bu 3 Inject SnCl into the reaction bottle, then inject 20ml of toluene solvent, and stir;
[0107] Inject 0.56ml (3.74mmol) of triethylamine into the reaction flask, and stir the reaction at 45°C for 6h to obtain the reaction product;
[0108] The reaction product was centrifuged, rotary evaporated, recrystallized in an ethanol solution of dichloromethane, and then vacuum-dried at 45°C to obtain the product, which was designated as Bu-Sn-POSS (Qt), and the yield was 85%. .
[0109] (1) Carry out infrared test to raw material Tetrasilanolpheny POSS and gained product, the infrared spectrogram that obtains is as follows figure 1 shown.
[0110] From figure 1 It can be seen that, compared with ...
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